Method of manufacturing spherical polymer particles from polymer solutions

• US 4,110,529 A
• Filed: 11/20/1975
• Issued: 08/29/1978
• Est. Priority Date: 11/26/1974
• Status: Expired due to Term

• Current Assignee: Ceschoslovak Akademie Ved
• Original Assignee: Ceschoslovak Akademie Ved
• Inventors: Stoy, Vladimir
• Primary Examiner(s): Lieberman, Allan
• Application Number:
  US05/633,787
• Time in Patent Office: 1,013 Days
• Field of Search: 260/34.2, 260/2.5 B, 260/2.5 A, 260/2 R, 260/2 EP, 260/75 T, 106/198, 106/122, 528/491, 528/492, 528/493, 528/494, 528/495, 528/496, 528/497, 528/498, 528/499, 528/502
• US Class Current: 528/491
• CPC Class Codes: A61K 9/1635 obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyvinyl pyrrolidone, poly(meth)acrylates
• CPC Class Codes: C08J 3/14 by precipitation from solutions C08J3/122 takes precedence

Abstract

The invention relates to a method of manufacturing spherical particles, either homogeneous or porous, from polymer solutions, wherein a polymer solution is dispersed or suspended in a liquid dispersing medium incapable of dissolving the polymer and immiscible with the polymer solvent, and the emulsion thus obtained is poured, while stirring, into an excess of a polymer-coagulating liquid which is miscible with the polymer solvent but immiscible with the dispersing medium, whereafter the two liquid phases are separated from each other and from the spherical polymer particles which are then isolated.

Claims

1. A method of forming a polymeric material into spherical particles or beads, which comprises providing a solution of the polymeric material in a solvent that dissolves the polymeric material without any chemical transformation of the latter;

dispersing the resulting polymeric material solution in a liquid dispersing medium that is a non-solvent for the polymeric material and is immiscible with the solvent, the volume ratio of the resulting dispersed phase to the dispersing medium varying from 1;

1 to 30;

1, the viscosity of the dispersing medium being no more than about one order less than the viscosity of the dispersed phase;

adding the resulting emulsion with stirring into an excess of a coagulating liquid that coagulates the polymeric material without any chemical transformation of the latter and that is a non-solvent for the polymeric material, is miscible with the solvent, and is immiscible with the dispersing medium;

whereupon the mixture is transformed directly into a three phase system of coagulated polymer, the coagulating liquid and the dispersing medium, and thereafter separating the liquid phases and resulting coagulated polymeric material particles or beads.

2. A method according to claim 1, in which the volume ratio of the dispersed phase to the dispersing medium ranges from 2:

1 to 15;

1.

3. A method according to claim 1, in which the polymeric material solution includes a liquid or solid additive that is dissolved or dispersed in such solution and that is insoluble in the dispersing medium and the coagulating liquid, such additive being incorporated in the resulting coagulated polymeric material particles or beads.

4. A method according to claim 3, which includes removing the additive from the coagulated polymeric material particles or beads.

5. A method according to claim 3, in which the dissolved or dispersed additive is such as to be coagulated by the coagulating liquid together with the polymeric material.

6. A method according to claim 5, which includes removing the additive from the coagulated polymeric material particles or beads.

7. A method according to claim 1, in which the polymeric material solution includes a solid additive that is dissolved or dispersed in such solution and that is insoluble in the dispersing medium but soluble in the coagulating liquid.

8. A method according to claim 1, in which the coagulating mixture includes a substance that reacts with the coagulated polymeric material to provide the latter with additional or new side groups.

9. A method according to claim 1, in which the coagulating liquid includes a minor proportion of the polymeric material solvent.

10. A method according to claim 9, which includes gradually adding further coagulating liquid to the coagulating mixture during the coagulation of the polymeric material.

11. A method according to claim 1, which includes cross-linking the polymeric material during or after coagulation of the same.

12. A method according to claim 1, which is carried out on a continuous basis.